Methyl iodide → HCID 59277705、化合物

HRID 1097774ノート

反応式

HRID 1097774 の反応式
I[CH3:2].[O:3]=[S:4]1(=[O:16])[CH2:9][C:8](=O)[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[N:5]1[CH3:15].[C:17]([O-:20])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:15][N:5]1[C:6]2[CH:7]=[CH:11][CH:12]=[CH:13][C:14]=2[C:17](=[O:20])[C:9]([CH3:8])([CH3:2])[S:4]1(=[O:3])=[O:16]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27375132,2-Dioxo-1-methyl-2,1-benzothiazin-4(3H)-one

生成物 1

HCID 59277705HCID 59277705、化合物収率 79.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

Iodomethane (187 ul, 426 mg, 3 mmol) is added dropwise to a suspension of 2,2-Dioxo-1-methyl-2,1-benzothiazin-4(3H)-one ([CAS: 7117-31-9], 220 mg, 1 mmol), K2CO3 (1.38 g, 10 mmol) in 3 mL of dry DMF at room temperature. The resulting mixture is stirred at 60° C. After 2 h, the reaction mixture is filtered, and washed with ethyl acetate (20 mL). The combined solution is concentrated and the residue is purified by flash column (ethyl acetate-heptane v/v 10%) and gives the title compound as white solid (190 mg).

後処理

  1. filtrationthe reaction mixture is filtered
  2. washwashed with ethyl acetate (20 mL)
  3. concentrationThe combined solution is concentrated
  4. customthe residue is purified by flash column (ethyl acetate-heptane v/v 10%)

出典と根拠

ORDレコード
ord-43d21b9309a547dc84ed1ec1af739cd5
出典データセット
uspto-grants-2012_03
特許番号
US08143278B2

反応ノート

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